EP3397596A1 - Use of magnesium hydroxide in the neutralization of pta wastewater - Google Patents

Use of magnesium hydroxide in the neutralization of pta wastewater

Info

Publication number
EP3397596A1
EP3397596A1 EP16826645.0A EP16826645A EP3397596A1 EP 3397596 A1 EP3397596 A1 EP 3397596A1 EP 16826645 A EP16826645 A EP 16826645A EP 3397596 A1 EP3397596 A1 EP 3397596A1
Authority
EP
European Patent Office
Prior art keywords
magnesium hydroxide
wastewater
effluent
mixing vessel
terephthalic acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP16826645.0A
Other languages
German (de)
English (en)
French (fr)
Inventor
Mamtu CHANDNANI
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BP Corp North America Inc
Original Assignee
BP Corp North America Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BP Corp North America Inc filed Critical BP Corp North America Inc
Publication of EP3397596A1 publication Critical patent/EP3397596A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/008—Control or steering systems not provided for elsewhere in subclass C02F
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/28—Anaerobic digestion processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/28—Anaerobic digestion processes
    • C02F3/2846—Anaerobic digestion processes using upflow anaerobic sludge blanket [UASB] reactors
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/30—Aerobic and anaerobic processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/74—Treatment of water, waste water, or sewage by oxidation with air
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/305—Endocrine disruptive agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/06—Controlling or monitoring parameters in water treatment pH

Definitions

  • the present invention relates to processes and apparatuses for the neutralization of wastewater containing terephthalic acid, and in particular, including the use of magnesium hydroxide to neutralize the wastewater.
  • Paraxylene is used to make purified terephthalic acid ("PTA").
  • Paraxylene is oxidized in the presence of a catalyst and an acetic acid solvent to make crude terephthalic acid.
  • the crude terephthalic acid is then hydrogenated to make PTA.
  • wastewater comprising organic materials terephthalic acid, acetic acid, para-to Ac acid
  • wastewater is neutralized by mixing the wastewater with a solution of diluted sodium hydroxide.
  • the mixing/neutralization occurs upstream of an anaerobic reactor in order to ensure that the wastewater is at the proper pH for the degradation of the terephthalic acid and other organic materials into methane, carbon dioxide, and water.
  • the present invention allows for greater control of the pH of the wastewater and thus the preservation of the activity in anaerobic biomass.
  • a process for treating wastewater comprising terephthalic acid.
  • the process comprises mixing magnesium hydroxide with wastewater comprising terephthalic acid in a mixing vessel to produce a neutralized wastewater effluent and removing organic material from the neutralized wastewater effluent in an anaerobic reactor.
  • an apparatus for treating wastewater comprising terephthalic acid comprises a source of wastewater comprising terephthalic acid, a source of magnesium hydroxide, a mixing vessel in fluid communication with the source of wastewater and the source of magnesium hydroxide, the mixing vessel adapted to mix the wastewater and the magnesium hydroxide to form a neutralized wastewater effluent, and an anaerobic reactor in fluid communication with the mixing zone, the anaerobic reactor comprising granules adapted remove organic material from the neutralized wastewater effluent.
  • Figure 1 is an apparatus for neutralizing wastewater comprising terephthalic acid using magnesium hydroxide
  • Figure 2 is an alternative embodiment of an apparatus for neutralizing wastewater comprising terephthalic acid using magnesium hydroxide.
  • Magnesium hydroxide is a much weaker base than sodium hydroxide.
  • using magnesium hydroxide as a pH control agent instead of sodium hydroxide minimizes pH spikes in the event of an inadvertent overdose of the pH control agent.
  • High doses of magnesium hydroxide in wastewater comprising terephthalic acid result in a maximum pH of 9.0 compared to high doses of sodium hydroxide, which result in a pH of up to 14.0.
  • magnesium hydroxide is used, recovery of biomass activity in an UASB reactor and the ability to degrade terephthalic acid is much quicker.
  • magnesium hydroxide recovery occurs in about three weeks compared to six to seven weeks when sodium hydroxide is use (plus permanent loss of the capability to degrade para-toluic acid).
  • Magnesium hydroxide acts a nutrient for anaerobic and aerobic systems, resulting in denser sludge in the clarifiers (the longer reaction time is conductive to crystal growth), cleaner water discharged, and sludge that is easier to dewater for disposal.
  • magnesium hydroxide has about 37 percent more hydroxide than sodium hydroxide, less magnesium hydroxide is required to neutralize a given amount of terephthalic acid.
  • Magnesium hydroxide is also non-hazardous by DOT standards.
  • magnesium hydroxide is non-corrosive, resulting in reduction in maintenance repair costs of valves, pipes, pumps, and storage tanks.
  • magnesium hydroxide takes longer to neutralize the terephthalic acid than sodium hydroxide.
  • a separate mixing vessel is required in order to allow about 20 minutes of residence time.
  • the mixing vessel requires an agitator.
  • FIG. 1 illustrates an apparatus 100 for treating wastewater comprising terephthalic acid.
  • the apparatus 100 comprises a source of wastewater comprising terephthalic acid, such as a process for making terephthalic acid 102 and a source of magnesium hydroxide, such as a tank 104 containing magnesium hydroxide and having an agitator 106 adapted to maintain the magnesium hydroxide in a slurry.
  • a source of wastewater comprising terephthalic acid such as a process for making terephthalic acid 102
  • a source of magnesium hydroxide such as a tank 104 containing magnesium hydroxide and having an agitator 106 adapted to maintain the magnesium hydroxide in a slurry.
  • the agitator may be a low revolutions per minute agitator, which keeps the slurry suspended in the tank 104.
  • the apparatus 100 also comprises a mixing vessel 108, which is in fluid communication with the source of wastewater comprising terephthalic acid 102 and the source of magnesium hydroxide 104.
  • the mixing vessel 108 is adapted to mix the wastewater and the magnesium hydroxide to form a neutralized wastewater effluent 110.
  • the apparatus 100 may also include a pump mechanism 112 adapted to pump magnesium hydroxide out of the tank 104, through a valve 114 in an inlet line 116, and into the mixing vessel 108.
  • the apparatus 100 further comprises an anaerobic reactor 118 in fluid communication with the mixing vessel 104.
  • the anaerobic reactor 118 may include granules 120 which are adapted to remove organic material from the neutralized wastewater effluent stream 110.
  • the anaerobic reactor may be, for example, an upflow anaerobic sludge blanket ("UASB"). Examples of organic material removed include terephthalic acid, acetic acid, and para-toluic acid.
  • the apparatus 100 may also comprise an aeration system 122 in fluid communication with the anaerobic reactor 118.
  • the aeration system 122 may be in fluid communication with the mixing vessel 108.
  • the aeration system 122 may be adapted to remove organic material from an effluent from the anaerobic reactor.
  • the apparatus 100 may further comprise a pH probe 124 configured to measure the pH of the neutralized wastewater effluent, and a dosing control mechanism adapted to control the amount of magnesium hydroxide introduced into the mixing vessel 108 based upon the measured pH.
  • the apparatus 100 may also comprise a flushing mechanism adapted to flush the inlet line with water to remove magnesium hydroxide therefrom.
  • the flushing mechanism may comprise a water line 126 and a flushing valve 128.
  • a process for treating wastewater comprising terephthalic acid is also provided.
  • Wastewater comprising terephthalic acid is introduced into the mixing vessel 108 through wastewater stream 130.
  • the wastewater stream may comprise about 650 ppm terephthalic acid.
  • Magnesium hydroxide is introduced into the mixing vessel 108 from the tank 104, through the inlet line 116.
  • Magnesium hydroxide and the wastewater comprising terephthalic acid are mixed in the mixing vessel 108 for a period of time to produce the neutralized wastewater effluent stream 1 10.
  • magnesium hydroxide and the wastewater are mixed for at least 20 minutes.
  • the neutralized wastewater effluent stream 1 10 is then introduced to the anaerobic reactor 118.
  • the pH of the neutralized wastewater stream 1 10 may be measured using pH probe 124. If the pH is less than a set point, additional magnesium hydroxide may be added through inlet line 1 16. If the pH is greater than a set point, the valve 1 14 in the inlet line 1 16 closes such that no magnesium hydroxide flows through inlet line 1 16. When the pH is greater than a set point, inlet line 1 16 may also be flushed with water through to remove any residual magnesium hydroxide and to prevent buildup of magnesium hydroxide in the inlet line 116. For example, when the pH is greater than a set point, valve 1 14 closes and flushing valve 128 opens, allowing water to flow through water line 126 through the inlet line 1 16 to the tank 104. Diameters of the pipes in the water line 126 and the inlet line 1 16 should allow for flow velocities of about 2 feet/second or more in order to prevent the magnesium hydroxide slurry from clogging the inlet line 116.
  • the anaerobic reactor produces a reactor effluent 132 and a biogas effluent 134.
  • the reactor effluent 132 from the anaerobic reactor 1 18 is substantially free of terephthalic acid.
  • Reactor effluent 132 may be returned to the mixing vessel 108, where it is further mixed with magnesium hydroxide to produce a second neutralized wastewater effluent stream 136.
  • the second neutralized wastewater effluent stream 136 may be introduced to an aeration system 122.
  • the aeration system 122 is adapted to remove remaining organic materials from the second neutralized wastewater effluent stream 136.
  • reactor effluent 132 may be directly introduced to the aeration system 122, as shown in Figure 2.
  • Mixing vessel 108 may be a mixing vessel in a wastewater treatment system.
  • mixing vessel 108 may be a sump or other collection basin in a process for making purified terephthalic acid, such as process 102.
  • Wastewater comprising terephthalic acid may be mixed with magnesium hydroxide in the mixing vessel, the sump, or both.
  • NaOH sodium sulfate
  • UASB reactor upflow anaerobic sludge blanket
  • Example 2 Mg(OH) 2 is introduced as an injection in a recirculation line instead of in the mixing vessel in order to determine the rate of reaction and pH control of the UASB reactor.
  • Example 3 Mg(OH) 2 is overfed to simulate a malfunction of the reactor effluent pH probe.
  • the feed mixture composition of a normal total organic carbon (“TOC”) wastewater stream and a high TOC wastewater stream is provided in Table 1 below.
  • a pilot plant mixing vessel is fed with a wastewater feed stream with a target TOC of 1155 ppm.
  • the wastewater feed pH is adjusted with a 61 weight percent Mg(OH) 2 slurry.
  • the amount of Mg(OH) 2 needed to increase the feed pH to 5.2 is about 80-85 grams. This is a reduction of 43-46 percent compared to the 148 grams of NaOH needed for the same feed.
  • the neutralized wastewater stream from the mixing vessel is then provided to the UASB reactor. pH of the effluent from the UASB reactor is about 6.6. Biogas release is constant and UASB reactor performance is also maintained at greater than 99 percent conversion of organic materials, with a slight gain in para-toluic acid conversion.
  • Mg(OH) 2 is diluted by 50 percent to a 30.5 weight percent slurry solution. The dilution reduces the pH range of the reactor effluent to between 6.4 and 7.1. With a 25 percent NaOH injection, the pH swing from 6.4 to 6.9. Biogas production also corresponds with pH swings with a drop in biog production due to higher solubility of CO2 in water at higher pH. Analysis of biog composition is shown in Table 2 below.
  • the UASB reactor is periodically fed with high TOCs and a new feed batch with high terephthalic acid, high acetic acid, and high total TOC of 1700 ppm is introduced to determine the control of effluent pH by Mg(OH)2 at high TOC loading rates.
  • Reactor TOC conversion is maintained at greater than 99 percent and the consumption of Mg(OH) 2 is 35-40 percent lower than that of NaOH at the same TOC loading rate.
  • the objective is to simulate malfunction of the pH probe, which would result in excess Mg(OH) 2 injection.
  • the Mg(OH) 2 pump is turned on for about 7 hours and 250 grams of Mg(OH) 2 is pumped to the UASB reactor (7 times the daily consumption of Mg(OH) 2 by the UASB reactor). pH peaks at about 8.2 and biogas production drops.
  • Analysis of the feed and effluent TOC indicates a drop in terephthalic acid and toluics conversion, but the remaining organic materials continued to degrade. Total TOC conversion dropped to 55 percent, but recovered within 72 hours to 90 percent conversion. However, conversion of toluics took about 21 days to achieve greater than 90 percent conversion.

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Removal Of Specific Substances (AREA)
  • Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
EP16826645.0A 2015-12-31 2016-12-28 Use of magnesium hydroxide in the neutralization of pta wastewater Withdrawn EP3397596A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201562273507P 2015-12-31 2015-12-31
PCT/US2016/068860 WO2017117211A1 (en) 2015-12-31 2016-12-28 Use of magnesium hydroxide in the neutralization of pta wastewater

Publications (1)

Publication Number Publication Date
EP3397596A1 true EP3397596A1 (en) 2018-11-07

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ID=57799920

Family Applications (1)

Application Number Title Priority Date Filing Date
EP16826645.0A Withdrawn EP3397596A1 (en) 2015-12-31 2016-12-28 Use of magnesium hydroxide in the neutralization of pta wastewater

Country Status (8)

Country Link
US (1) US20170190604A1 (ko)
EP (1) EP3397596A1 (ko)
KR (1) KR20180098348A (ko)
CN (1) CN109071284A (ko)
BR (1) BR112018013047A2 (ko)
MX (1) MX2018007990A (ko)
RU (1) RU2018127205A (ko)
WO (1) WO2017117211A1 (ko)

Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN111762981A (zh) * 2020-07-21 2020-10-13 新疆中泰创新技术研究院有限责任公司 Pta污水处理系统及处理方法

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CN110180492B (zh) * 2019-04-17 2022-09-23 中节能（合肥）可再生能源有限公司 一种用于去除镁离子的活性滤料及其制备方法和应用
CN110066049A (zh) * 2019-05-14 2019-07-30 杭州汇维仕永盛染整有限公司 一种碱减量废水中pta的回收工艺及系统
CN111392974A (zh) * 2020-04-12 2020-07-10 嘉兴晟景环境科技有限公司 一种高pta废水厌氧深度处理装置及方法
CN111689654A (zh) * 2020-06-30 2020-09-22 新疆中泰创新技术研究院有限责任公司 能够减少pta厌氧污泥投加的污水处理系统及方法
FR3143590A1 (fr) * 2022-12-15 2024-06-21 Timab Magnesium Utilisation d’hydroxyde de magnésium pour accélérer la cinétique de production de biogaz dans un digesteur anaérobie
FR3143591A1 (fr) * 2022-12-15 2024-06-21 Timab Magnesium Utilisation d’hydroxyde de magnésium dans un digesteur anaérobie

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Also Published As

Publication number Publication date
CN109071284A (zh) 2018-12-21
US20170190604A1 (en) 2017-07-06
WO2017117211A1 (en) 2017-07-06
MX2018007990A (es) 2018-11-09
RU2018127205A (ru) 2020-01-31
BR112018013047A2 (pt) 2018-12-04
KR20180098348A (ko) 2018-09-03

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